CN115260763A - Polyimide black film with high insulation strength and preparation method thereof - Google Patents
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Abstract
The invention discloses a polyimide black film with high insulation strength and a preparation method thereof. The polyimide black film is composed of a polyimide matrix and a carbon-based nano composite filler, wherein the carbon-based nano composite filler has a core-shell structure, carbon nanoparticles are taken as a core, and polymer or/and inorganic nanoparticles are taken as a functional shell layer, wherein the carbon nanoparticles are combined with the polymer or/and the inorganic nanoparticles through van der Waals force, electrostatic force, hydrogen bonds or pi-pi conjugation. The preparation process comprises the steps of preparing carbon nano particles and carbon-based nano composite filler with a core-shell structure, introducing the carbon-based nano composite filler into a polyimide precursor solution, coating a gel film on a planar substrate, and curing and imidizing to finally obtain a target product. The composite film has high electric insulation strength, light shading property, heat conducting property, thermal stability, dimensional stability and photo-thermal conversion property, and has high application value in the field of electronic packaging.
Description
Technical Field
The invention belongs to the technical field of films, and particularly relates to a polyimide black film with high insulation strength and a preparation method thereof.
Background
Polyimide films (PIs) have been widely used in the field of electronic packaging due to excellent heat resistance, chemical resistance, strong mechanical properties, and excellent flexibility. With the rise of the electronic industry, the demand of electronic-grade black polyimide covering films is sharply increased. The black polyimide cover film mainly plays a role in packaging and covering flexible circuits and electronic components, avoids the influence of negative factors such as dust and water vapor and prevents visual inspection, tampering and plagiarism. Currently, the common polyimide black film on the market is dyed mainly by introducing carbon black into a polyimide matrix, which is mainly due to the low cost and good dyeing property of the carbon black. However, the intrinsic high insulation performance of the polyimide film is greatly reduced by the excellent conductivity of the carbon black, and the requirement of customers for electrical insulation performance cannot be met. In addition, as electronic packaging technology is developed towards thinning, integration and multi-functionalization, the wiring density and power consumption of a chip are increased sharply, so that a large amount of joule heat generation and accumulation are generated and generated in the operation process of an electronic device, and the reliability, safety and durability of the electronic device are seriously damaged when the electronic device is in an overheat environment for a long time. The polyimide cover film is used as a packaging material of the electronic component and plays an important role in rapid heat dissipation of the electronic component. However, polyimide films, like other hydrocarbon-based polymers, have severe phonon scattering in the amorphous regions and interfaces, resulting in low intrinsic thermal conductivity, on the order of 0.2Wm -1 K -1 And the requirement of rapid heat dissipation of electronic components cannot be met.
Disclosure of Invention
One of the purposes of the invention is to provide a polyimide black film with high insulation strength for overcoming the defects of low thermal conductivity and poor insulation performance of polyimide cover films in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a polyimide black film with high insulation strength is composed of a polyimide matrix and carbon-based nano composite fillers uniformly dispersed in the polyimide matrix, wherein the mass ratio of the polyimide matrix to the carbon-based nano composite fillers is (0.1-100), the carbon-based nano composite fillers are of a core-shell structure, a core is carbon nanoparticles, a functional shell layer coated on the outer layer of the core is polymer or/and inorganic nanoparticles, the mass ratio of the carbon nanoparticles, the polymer or/and the inorganic nanoparticles is (1) (0.1-3), and the carbon nanoparticles, the polymer or/and the inorganic nanoparticles are combined through one or more of van der Waals force, electrostatic force, hydrogen bonds or pi-pi conjugation.
Further improvement as a polyimide black film having high insulation strength:
preferably, the carbon nanoparticles are formed by combining one or more than two of single carbon microspheres and interconnections consisting of more than two carbon microspheres, and the diameters of the carbon microspheres are 200-800nm.
Preferably, the polymer is one or more than two of polydopamine, alginic acid, alginate, chitosan, a silane coupling agent and polyacrylic acid, and the inorganic nanoparticles are one or more than two of carbon nitride nanosheets, boron nitride nanotubes, silicon dioxide, silicon carbide, aluminum nitride and aluminum oxide.
The second purpose of the invention is to provide a preparation method of the polyimide black film with high insulation strength, which comprises the following steps:
s1, dispersing a carbon nano particle precursor into water according to the mass ratio of (3-10) to 60, fully stirring and dissolving, transferring into a high-temperature high-pressure reaction kettle, and carrying out programmed heating treatment, wherein the heating program is as follows: heating to 150-240 ℃ from room temperature at a heating rate of 1-10 ℃/min, keeping the temperature for 0.5-5h, cooling to room temperature after the reaction is finished, separating solid precipitate, and drying to obtain carbon nanoparticles;
s2, weighing 100 parts by mass of carbon nano particles, uniformly dispersing the carbon nano particles in 200-500 parts by mass of water, adding 10-300 parts by mass of polymer or/and inorganic nano particles, after fully stirring, separating out solid precipitate and drying to prepare the carbon-based nano composite filler;
or weighing 100 parts by mass of the carbon nanoparticles prepared in the step S1, uniformly dispersing the carbon nanoparticles in 200-500 parts by mass of water, adding 100-1000 parts by mass of a carbon nitride precursor, fully stirring, separating out a solid precipitate, drying, transferring the obtained solid powder to a tubular furnace, and heating by a preset program under the protection of inert atmosphere: heating to 400-650 ℃ from room temperature at a heating rate of 1-10 ℃/min, and keeping the temperature for 1-5h to prepare the carbon-based nano composite filler;
s3, weighing 1-100 parts by mass of carbon-based nano composite filler, uniformly dispersing the carbon-based nano composite filler in 500-1000 parts by mass of aprotic polar solvent, adding 100 parts by mass of polyimide precursor, fully stirring to obtain uniformly mixed colloidal solution, defoaming, transferring the colloidal solution onto a planar substrate by adopting a film forming process, and curing and imidizing to obtain the polyimide black film with high insulating strength.
As a further improvement of the preparation method of the polyimide black film having high insulation strength:
preferably, the carbon nanoparticle precursor in step S1 is one or a combination of two or more of glucose, chitosan, fructose, sucrose, starch, vegetable oil, succinic acid, citric acid, and lactic acid.
Preferably, solid precipitates are separated in the steps S1 and S2 through vacuum filtration or high-speed centrifugation, the rotation speed of the high-speed centrifugation is 500-10000 circles/min, and the temperature of the drying treatment is 60-150 ℃.
Preferably, in step S2, the carbon nitride precursor is one or a combination of two or more of cyanamide, dicyanamide and melamine, and the inert atmosphere is one of nitrogen, argon and helium.
Preferably, the aprotic polar solvent in step S3 is N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, or dimethylsulfoxide.
Preferably, the polyimide precursor in step S3 is polyamic acid obtained by polymerizing dianhydride and diamine, or polyamic acid obtained by polymerizing dianhydride and diamine.
Preferably, the specific procedures of curing and imidizing in step S3 are: heating from room temperature at 1-5 deg.C/min to 300-400 deg.C, and maintaining at the temperature for 0-60min.
Compared with the prior art, the invention has the beneficial effects that:
1) Tests show that the polyimide black film with high insulation strength has excellent heat conduction performance, the heat conduction rate is respectively improved by 8-20 times and 2-6 times in the horizontal direction and the vertical direction under the filling of lower carbon-based nano composite filler, the polyimide black film simultaneously shows rapid photo-thermal generating capacity under the irradiation of sunlight, and the obtained polyimide black film keeps inherent electrical insulation, thermal stability and dimensional stability. The polyimide black film with high insulation strength has high application value in the field of electronic packaging.
2) The preparation method of the polyimide black film with high insulation strength overcomes the defects that the prior art cannot simultaneously improve the heat conductivity in the horizontal and vertical directions and the intrinsic excellent electrical insulation performance of the polymer matrix is lost due to the use of the carbon-based material, and the carbon nanoparticles are wrapped by using the polymer or/and the inorganic nanoparticles as the functional shell material for the first time, so that the carbon-based nano composite filler has high heat conductivity and excellent electrical insulation performance; the preparation process is simple to operate, the reagents participating in the reaction are green and environment-friendly, the preparation process does not involve harsh reaction conditions, and large-scale mass production of the polyimide black film with high insulation strength is easy to realize.
Drawings
Fig. 1 (a) is a projection electron microscope (TEM) picture of carbon nanoparticles prepared in example 1 of the present invention; fig. 1 (b) is a projection electron microscope (TEM) image of the carbon-based nanocomposite filler prepared in example 1 of the present invention; fig. 1 (c) is a Scanning Electron Microscope (SEM) picture of a cross section of a polyimide black film having high dielectric strength.
FIG. 2 shows the electrical insulation test of pure polyimide films and polyimide black films having high insulation strength obtained in examples 1 to 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative effort based on the embodiments of the present invention belong to the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of a polyimide black film with high insulation strength, which comprises the following steps:
(1) Weighing 10g of glucose, adding the glucose into 60mL of deionized water, fully stirring and dissolving, transferring the glucose into a 100mL high-temperature high-pressure reaction kettle, further placing the reaction kettle in a high-temperature oven, heating the reaction kettle from room temperature to 200 ℃ at the heating rate of 2 ℃/min, preserving the heat at the temperature for 3h, naturally cooling the reaction kettle to the room temperature, cleaning the obtained product in a vacuum filtration mode, further placing the obtained product in a vacuum oven at 80 ℃ for drying for 4h, and finally obtaining the carbon nanoparticles.
(2) Weighing 100g of carbon nano particles, uniformly dispersing the carbon nano particles in 300mL of deionized water, then adding 300g of melamine, stirring for 24 hours to ensure the sufficient interaction of the carbon nano particles and the melamine, then separating out a precipitate through vacuum filtration, and further placing the precipitate in a vacuum oven at 100 ℃ for drying; and (3) transferring the dried precipitate into a tubular furnace, heating from room temperature to 600 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, preserving heat for 5 hours at the temperature, and cooling to room temperature after the reaction is finished to obtain the carbon-based nano composite filler.
(3) Weighing 0.87g of carbon-based nano composite filler, uniformly dispersing the carbon-based nano composite filler into 11.6g of N, N-dimethylacetamide, then adding 1g of 4,4 '-diaminodiphenyl ether, stirring for 30min until 4,4' -diaminodiphenyl ether is completely dissolved, then adding 1.04g of pyromellitic dianhydride, continuously stirring for 2h, standing the colloidal solution for 30min to remove bubbles after stirring is finished, then uniformly coating the colloidal solution on a glass substrate by using a coating machine, immediately placing the glass substrate in a high-temperature oven, heating from room temperature to 350 ℃ at the heating rate of 3 ℃/min for curing and imidization, and cooling to room temperature to obtain the polyimide black film with high insulation strength.
Scanning electron microscope testing is carried out on the carbon nano particles prepared in the step (1), and the result is shown in figure 1 (a); performing scanning electron microscope test on the carbon-based nano composite filler prepared in the step (2), wherein the result is shown in fig. 1 (b); scanning electron microscope testing is carried out on the cross section of the polyimide black film with high insulating strength prepared in the step (3), and the result is shown in figure 1 (b); FIG. 1 (a) shows that the diameter of the carbon microsphere is about 300nm, and the carbon nanoparticle is an interconnected body of two or more carbon microspheres and has a smooth surface; in fig. 1 (b), it is apparent that the surface of the carbon nanoparticles becomes rough, and the carbon nitride is uniformly coated on the surface of the carbon nanoparticles. In fig. 1 (c), it can be seen that the carbon-based nanocomposite filler is uniformly distributed in the polyimide matrix, which is attributed to the good compatibility of the carbon-based nanocomposite filler modified by carbon nitride with the polyimide matrix.
Example 2
The preparation method was the same as example 1 except that the amount of the carbon-based nanocomposite filler added in step (3) was adjusted to 0.51g and the amount of N, N-dimethylacetamide was adjusted to 10.2mL, as a comparative example for example 1.
Example 3
The preparation method was the same as example 1 except that the amount of the carbon-based nanocomposite filler added in step (3) was adjusted to 0.23g and the amount of N, N-dimethylacetamide was adjusted to 9.06mL, which was regarded as a comparative example of example 1.
Example 4
The preparation method was the same as example 1 except that the amount of the carbon-based nanocomposite filler added in step (3) was adjusted to 0.11g and the amount of N, N-dimethylacetamide was adjusted to 8.6mL, as a comparative example for example 1.
Example 5
The preparation method is referred to as example 1, except that the specific steps of the step (2) are as follows:
weighing 100g of carbon nanoparticles, uniformly dispersing in 300mL of deionized water, adding 300g of polydopamine, stirring for 24h to ensure that the carbon nanoparticles and the polydopamine are fully interacted, then separating out a precipitate through vacuum filtration, and further placing the precipitate in a vacuum oven at 100 ℃ for drying to obtain the carbon-based nano composite filler, which is used as a comparative example of example 1.
The polyimide black films having high dielectric strength prepared in examples 1 to 4 were respectively tested for electrical insulation and thermal conductivity, and the results are shown in fig. 2 and table 1.
As shown in fig. 2, although the volume resistivity of the polyimide black film is reduced as the addition amount of the carbon-based nanocomposite filler is increased, it maintains excellent electrical insulation property, which is benefited from the formation of conductive paths between carbon nanoparticles blocked by the polymer or/and inorganic nanoparticles as shell materials.
The thermal conductivity of the pure polyimide film and the polyimide black film with different carbon-based nanocomposite filler addition amounts are shown in table 1 below.
TABLE 1 Heat transfer Performance testing of pure polyimide films and polyimide Black films of examples 1-4
| Sample (I) | Horizontal thermal conductivity (Wm) -1 K -1 ) | Vertical thermal conductivity (Wm) -1 K -1 ) |
| Pure polyimide film | 0.18 | 0.18 |
| Example 1 | 1.98 | 0.43 |
| Example 2 | 1.51 | 0.32 |
| Example 3 | 1.06 | 0.25 |
| Example 4 | 0.75 | 0.21 |
| Example 5 | 0.93 | 0.27 |
As can be seen from Table 1, the pure polyimide film exhibited a low intrinsic thermal conductivity of about 0.18Wm, similar to other hydrocarbon-based polymers -1 K -1 . Then after the carbon-based nano composite filler is introduced, the thermal conductivity of the polyimide film is greatly improved, and the polyimide film has obvious anisotropy, which shows that the prepared carbon-based nano composite filler has great heat conduction enhancement potential. If the content of the carbon-based nano composite filler is 30wt%, the thermal conductivity of the polyimide film in the horizontal direction and the vertical direction respectively reaches 1.98 and 0.43Wm -1 K -1 . Along with the reduction of the addition amount of the carbon-based nano composite filler, the horizontal and vertical thermal conductivity of the polyimide film is reduced, but the horizontal and vertical thermal conductivity of the polyimide film is higher than that of a pure polyimide film. Meanwhile, the composite film has high light-shielding property, thermal stability and photo-thermal conversion performanceAnd electrical insulation, and has high practical value in the field of packaging.
It should be understood by those skilled in the art that the foregoing is only illustrative of several embodiments of the invention, and is not an exhaustive list. It should be noted that many variations and modifications are possible to those skilled in the art, and it is intended to cover all such variations and modifications that fall within the scope of the appended claims.
Claims (10)
1. The polyimide black film with high insulation strength is characterized by comprising a polyimide matrix and carbon-based nano composite fillers uniformly dispersed in the polyimide matrix, wherein the mass ratio of the polyimide matrix to the carbon-based nano composite fillers is (0.1-100), the carbon-based nano composite fillers are of a core-shell structure, the core is carbon nanoparticles, the functional shell layer coated on the outer layer of the core is polymer or/and inorganic nanoparticles, the mass ratio of the carbon nanoparticles, the polymer or/and the inorganic nanoparticles is (1) (0.1-3), and the carbon nanoparticles, the polymer or/and the inorganic nanoparticles are combined through one or more than two of van der Waals force, hydrogen bond, electrostatic force or pi-pi conjugation.
2. The polyimide black film with high dielectric strength as claimed in claim 1, wherein the carbon nanoparticles are formed by combining one or more of a single carbon microsphere and an interconnection body formed by two or more carbon microspheres, and the diameter of the carbon microsphere is 200-800nm.
3. The polyimide black film with high dielectric strength as claimed in claim 1 or 2, wherein the polymer is one or more of polydopamine, alginic acid, alginate, chitosan, silane coupling agent and polyacrylic acid, and the inorganic nanoparticles are one or more of carbon nitride nanosheets, boron nitride nanotubes, silica, silicon carbide, aluminum nitride and aluminum oxide.
4. A method for preparing a polyimide black film with high dielectric strength according to any one of claims 1 to 3, comprising the steps of:
s1, dispersing a carbon nano particle precursor into water according to the mass ratio of (3-10) to 60, fully stirring and dissolving, transferring into a high-temperature high-pressure reaction kettle, and carrying out programmed heating treatment, wherein the heating program is as follows: heating to 150-240 ℃ from room temperature at a heating rate of 1-10 ℃/min, keeping the temperature for 0.5-5h, cooling to room temperature after the reaction is finished, separating solid precipitate, and drying to obtain carbon nanoparticles;
s2, weighing 100 parts by mass of carbon nano particles, uniformly dispersing the carbon nano particles in 200-500 parts by mass of water, adding 10-300 parts by mass of polymer or/and inorganic nano particles, fully stirring, separating out solid precipitate, and drying to obtain the carbon-based nano composite filler;
or weighing 100 parts by mass of the carbon nanoparticles prepared in the step S1, uniformly dispersing the carbon nanoparticles in 200-500 parts by mass of water, adding 100-1000 parts by mass of a carbon nitride precursor, fully stirring, separating out a solid precipitate, drying, transferring the obtained solid powder to a tubular furnace, and heating by a preset program under the protection of inert atmosphere: heating to 400-650 ℃ from room temperature at a heating rate of 1-10 ℃/min, and keeping the temperature for 1-5h to prepare the carbon-based nano composite filler;
s3, weighing 1-100 parts by mass of carbon-based nano composite filler, uniformly dispersing the carbon-based nano composite filler in 500-1000 parts by mass of aprotic polar solvent, adding 100 parts by mass of polyimide precursor, fully stirring to obtain a uniformly mixed colloidal solution, defoaming, transferring the colloidal solution onto a planar substrate by adopting a film forming process, and curing and imidizing to obtain the polyimide black film with high insulating strength.
5. The method for preparing a polyimide black film with high dielectric strength according to claim 4, wherein the carbon nanoparticle precursor in step S1 is one or a combination of two or more of glucose, chitosan, fructose, sucrose, starch, vegetable oil, succinic acid, citric acid, and lactic acid.
6. The method for preparing polyimide black film with high dielectric strength as claimed in claim 4, wherein the solid precipitate is separated in steps S1 and S2 by vacuum filtration or high speed centrifugation at 500-10000 circles/min and the temperature of drying treatment is 60-150 ℃.
7. The method for preparing the polyimide black film with high dielectric strength according to claim 4, wherein the carbon nitride precursor in step S2 is one or a combination of two or more of cyanamide, dicyanamide and melamine, and the inert atmosphere is one of nitrogen, argon and helium.
8. The method for preparing the polyimide black film with high dielectric strength as claimed in claim 4, wherein the aprotic polar solvent in step S3 is N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, or dimethylsulfoxide.
9. The method for preparing the polyimide black film with high dielectric strength according to claim 4, wherein the polyimide precursor in the step S3 is polyamic acid obtained by polymerizing dianhydride and diamine, or polyamic acid obtained by polymerizing dianhydride and diamine.
10. The method for preparing the polyimide black film with high dielectric strength as claimed in claim 4, wherein the curing and imidizing in step S3 are carried out by the following specific procedures: heating from room temperature at 1-5 deg.C/min to 300-400 deg.C, and maintaining at the temperature for 0-60min.
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Cited By (2)
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| CN117777548A (en) * | 2023-12-04 | 2024-03-29 | 科迈特新材料有限公司 | Modified flame retardant for high polymer material and preparation method thereof |
| CN117777548B (en) * | 2023-12-04 | 2024-05-31 | 科迈特新材料有限公司 | Modified flame retardant for high polymer material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102509A (en) * | 2013-01-22 | 2013-05-15 | 太原理工大学 | Core-shell type carbon microspheres and preparation method and application thereof |
| CN106189012A (en) * | 2016-07-08 | 2016-12-07 | 西北工业大学 | A kind of polymer matrix composite and preparation method thereof |
| CN109319760A (en) * | 2018-11-12 | 2019-02-12 | 青岛科技大学 | A kind of carbon micron-spheres and preparation method thereof |
| CN110628158A (en) * | 2019-09-27 | 2019-12-31 | 陕西科技大学 | Aqueous phase free radical polymerization preparation method of polymethyl methacrylate/carbon microsphere nano composite material with core-shell structure |
| CN111471299A (en) * | 2020-06-01 | 2020-07-31 | 中国科学院合肥物质科学研究院 | Heat-conducting and insulating polyimide nano composite film and preparation method thereof |
| CN114455567A (en) * | 2020-11-03 | 2022-05-10 | 广东量子墨滴生物科技有限公司 | Preparation method and application of carbon nanoparticles |
-
2022
- 2022-09-06 CN CN202211083265.3A patent/CN115260763B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102509A (en) * | 2013-01-22 | 2013-05-15 | 太原理工大学 | Core-shell type carbon microspheres and preparation method and application thereof |
| CN106189012A (en) * | 2016-07-08 | 2016-12-07 | 西北工业大学 | A kind of polymer matrix composite and preparation method thereof |
| CN109319760A (en) * | 2018-11-12 | 2019-02-12 | 青岛科技大学 | A kind of carbon micron-spheres and preparation method thereof |
| CN110628158A (en) * | 2019-09-27 | 2019-12-31 | 陕西科技大学 | Aqueous phase free radical polymerization preparation method of polymethyl methacrylate/carbon microsphere nano composite material with core-shell structure |
| CN111471299A (en) * | 2020-06-01 | 2020-07-31 | 中国科学院合肥物质科学研究院 | Heat-conducting and insulating polyimide nano composite film and preparation method thereof |
| CN114455567A (en) * | 2020-11-03 | 2022-05-10 | 广东量子墨滴生物科技有限公司 | Preparation method and application of carbon nanoparticles |
Non-Patent Citations (1)
| Title |
|---|
| 王艳艳: ""聚酰亚胺/氮化碳纳米复合薄膜的微观结构设计与导热性能研究"", 中国博士学位论文全文数据库（电子期刊） * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117777548A (en) * | 2023-12-04 | 2024-03-29 | 科迈特新材料有限公司 | Modified flame retardant for high polymer material and preparation method thereof |
| CN117777548B (en) * | 2023-12-04 | 2024-05-31 | 科迈特新材料有限公司 | Modified flame retardant for high polymer material and preparation method thereof |
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